Development of a dispersive liquid–liquid microextraction method for the simultaneous determination of the main compounds causing cork taint and Brett character in wines using gas chromatography–tandem mass spectrometry

Abstract

A novel dispersive liquid–liquid microextraction (DLLME) method, coupled to gas chromatography–tandem mass spectrometry (GC–MS/MS), was developed for simultaneously determining the main compounds responsible for cork taint (2,4,6-trichloranisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and pentachloranisole (PCA)) and Brett character (4-ethylguaiacol (EG), 4-ethylphenol (EP), 4-vinylguaiacol (VG) and 4-vinylphenol (VP)) in wines. Optimisation of DLLME procedure was performed by evaluating the type of disperser and extraction solvents and the temperature and salt addition effects. The volumes of disperser and extraction solvents were also optimised by means of a central composite design combined with desirability functions. Under optimum conditions, 5 mL of wine were extracted with an extraction mixture consisting of 1.43 mL of acetone, and 173 μL of chloroform at room temperature. The analytical characteristics of the method were evaluated. Satisfactory linearity (with correlation coefficients over 0.992), repeatability (below 11.6%) and between-days precision (below 11.0%) were obtained for all target analytes. Detection limits attained were at similar levels or even lower than the olfactory threshold of the studied compounds. Finally, the developed method was successfully applied to the analysis of wine samples. To our knowledge, this is the first time that DLLME has been applied to simultaneously determine the compounds responsible for cork taint and Brett character in wine.